| The technical contribution of this research is a unique nanofabricated experimental setup that integrates nanoscale specimens with tools for interrogating mechanical (stress-strain, fracture, and fatigue), thermal and electrical (conductivity) properties as function of external stimuli such as strain, temperature, electrical field and radiation. It addresses the shortcomings of the state of the art characterization techniques, which are yet to perform such simultaneous and multi-domain measurements. Our technique has virtually no restriction on specimen material type and thickness, which makes the setup versatile. It is demonstrated with 100 nm thick nickel, aluminum, zirconium; 25 nm thick molybdenum di-sulphide (MoS2), 10 nm hexagonal boron nitride (h-BN) specimens and 100nm carbon nanofiber, all in freestanding thin film form. The technique is compatible with transmission electron microscopy (TEM). In-situ TEM captures microstructural features, (defects, phases, precipitates and interfaces), diffraction patterns and chemical microanalysis in real time. 'Seeing the microstructure while measuring properties' is our unique capability. It helps identifying fundamental mechanisms behind thermo-electro-mechanical coupling and degradation, so that these mechanisms can be used to (i) explain the results obtained for mesoscale specimens of the same materials and experimental conditions and (ii) develop computational models to explain and predict properties at both nano and meso scales. The uniqueness of this contribution is therefore simultaneously quantitative and qualitative probing of length-scale dependent external stimuli effects on microstructures and physical properties of nanoscale materials.;The scientific contribution of this research is the experimental validation of the fundamental hypothesis that, if the nanoscale size can cause significant deviation in a certain domain, e.g., mechanical, it can also make that domain more sensitive to external stimuli when compared to bulk. We have showed that mechanical properties of freestanding nanocrystalline thin films have higher sensitivity to elevated temperatures compared to bulk. The Young's modulus of nanocrystalline aluminum thin film is measured about 50% of the room temperature value at 65% of the melting temperature. The higher volume fraction of grain boundaries can be ascribed to this observation since the inherent disorder on the grain boundary atoms means they are more sensitive to the temperature. At the bulk scale, thermal conductivity of metals is not sensitive to mechanical strain. However, this may not be true for grain sizes below the electron mean free paths, for which mechanical deformation mechanism and volume fraction of grain boundaries are drastically different from the bulk. Our experimental results show strong mechanical strain-thermal conductivity coupling, thermal conductivity of Zr film with average grain size of 10nm dropped from 20 W/m-K to 13 W/m-K with a strain level of only 1.24 %.;In this dissertation, we present a series of studies tied by the common thread of synergy of two or more stimuli. The first example is on pure metals, which need very high temperature (> 0.5Tm, where Tm is melting point) or stress (>sigmay, where sigmay is the yield stress) to change microstructure. In contrast, we present experimental evidence of about 100 times grain growth in nanocrystalline nickel at only 0.2Tm (Tm is the melting temperature) when accompanied with only 0.2 sigmay ( sigmay is the yield stress) stress. This finding contradicts with the classical understanding that grain growth is a plastic deformation (>sigmay) mechanism. Interestingly, stressing the films by high stress (around sigmay) or temperature (0.5Tm) separately produce only insignificant grain growth. These results suggest that when synergistic, external stimuli can exert unprecedented influence over microstructure-properties in nanoscale materials. In a corollary study, we modeled nanocrystalline metals as a standard linear elastic solid and our experimental results on 100 nm thick (average grain size 10 nm) freestanding nickel specimens at temperatures from 300 to 425 °K support this hypothesis reasonably well. The viscosity of solid nickel ranged from 3.3x1013 Pa.s to 1.5x1013 Pa.s at these temperatures, which are about two orders of magnitude smaller than that expected for metals and are also less sensitive to temperature compared to bulk.;The second case study involved a novel concept of electro-graphitization that induces synergistic thermo-electro-mechanical fields to graphitize carbon nanofibers at around 800 °C temperature and below 106 A/cm 2 current density. In comparison, conventional graphitization of carbon nanofiber requires very high temperatures (> 2800 °C). A more convincing study on the pronounced role of stimuli on microstructure-properties is the transformation of amorphous materials to nano or microcrystalline form. This is because typically the energy barrier for this kind of transformation is very high, requiring extreme conditions to initiate such transformation. (Abstract shortened by ProQuest.). |
